CN101298347B - Covalent bond type inorganic organic composite flocculant, preparation process and use thereof - Google Patents
Covalent bond type inorganic organic composite flocculant, preparation process and use thereof Download PDFInfo
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- CN101298347B CN101298347B CN2008101159908A CN200810115990A CN101298347B CN 101298347 B CN101298347 B CN 101298347B CN 2008101159908 A CN2008101159908 A CN 2008101159908A CN 200810115990 A CN200810115990 A CN 200810115990A CN 101298347 B CN101298347 B CN 101298347B
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Abstract
The invention relates to a covalent bond type inorganic/organic compound flocculant, a production technique and an application thereof. The invention adopts Gamma-APDES (gamma-Aminopropylmethyldiethoxysilane) and aluminum chloride solution as the raw materials to produce the covalent bond type inorganic/organic compound flocculant by gradually dripping alkaline. The a covalent bond type inorganic/organic compound flocculant, the production technique and the application thereof have the advantages that the inorganic constituent and the organic constituent in the flocculant are bonded by covalent bond, which has good stability, good turbidity removal and decoloration effect and wider optimal dosing range. The covalent bond type inorganic/organic compound flocculant can be used for the waterpurification and the turbidity removal, decoloration, deoiling and solid-liquid separation during the wastewater treatment.
Description
Technical field
The invention belongs to the synthesis technical field of polymeric flocculant in the water treatment field, specifically, the present invention relates to a kind of covalent bond type inorganic organic composite flocculant, preparation technology and application thereof.
Background technology
Coagulation process is most widely used general, a most general unit operation technology in the engineering of water treatment.The coagulating treatment effect is directly determining operation condition, final outflow water quality and the cost of follow-up processing flow.The flocculating effect quality depends on flocculation agent to a great extent.Inorganic polymer flocculant and organic polymer coargulator are to use two more class flocculation agents in the current water treatment.The inorganic polymer flocculant price is relatively cheap, but it is low to have a molecular weight, and is poor at water stability, and the dosage height produces shortcomings such as sludge quantity is big.Organic polymer coargulator has that functional group is many, and molecular weight is big, and consumption is few, and settling velocity is fast, and is applied widely, and sludge quantity is few and be easy to advantages such as dehydration; Shortcoming is that price is higher, to removal ability than fine particle, and best dispensing narrow range, not easy to operate etc.Be comprehensive the two advantage, the normal method that adopts substep to add in the water treatment procedure, will be inorganic with the organic polymer coargulator coupling to reach treatment effect preferably.Though this has reached the purpose of having complementary advantages to a certain extent, the consequent is that operating procedure is loaded down with trivial details, and facility investment is big, and use cost is higher relatively etc.Based on this, inorganic organic composite coagulator arises at the historic moment, it not only can reach and add inorganic and the equal even better flocculating effect of organic floculant with substep, and, on the basis of improving processing efficiency, equipment investment cost and cost for wastewater treatment have been reduced because operating procedure has been simplified in disposable dosing.
At present, the compound inorganic flocculating agent and the organic polymer coargulators such as aluminium system, iron system, iron aluminium system, polysilicate of mainly concentrating on of inorganic and organic floculant are as the various combination between chitin, polyacrylamide (PAM), the dimethyl diallyl ammonium chloride (PDMDAAC) etc.As preparing inorganic organic composite coagulator with polymerize aluminum chloride and chitosan among the patent CN1266821A; Prepare inorganic organic composite coagulator with the polymkeric substance of Dicyanodiamide and formaldehyde, poly-sulphur aluminum chloride and poly-sulphur aluminum calcium chloride among the patent CN1393410A; Adopt acrylamide, N among the patent CN1554592A, N-dimethyl diallyl ammonium chloride or (methyl) acrylyl oxy-ethyl-trimethyl salmiac and aluminium hydroxide (ironic hydroxide, magnesium hydroxide, zinc hydroxide) preparation inorganic organic composite coagulator; Then adopt polymeric aluminum and dimethyl diallyl ammonium chloride to prepare inorganic organic composite coagulator among the patent CN1594128A; Raw material is polymerization iron and dimethyl diallyl ammonium chloride among the patent CN1724404A.But in this class composite flocculation agent " compound " of inorganic component and organic constituent, only combine, be difficult to keep the stability of flocculation agent, thereby the application of influence in actual water treatment by coordination or electrostatic interaction loosely.Therefore this class flocculation agent can only be called " composite " strictly speaking, rather than truly " compound ".Should exist the covalent linkage that connects inorganic component and organic constituent in the real compound inorganic organic composite coagulator, i.e. covalent bond type inorganic organic composite flocculant.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, and a kind of covalent bond type inorganic organic composite flocculant, preparation technology and application thereof are provided.
The present invention seeks to realize by following measure: (molecular formula is NH for γ-Aminopropylmethyldiethoxysilane, APDES with γ-aminopropyl diethoxymethyl silane in the present invention
2C
3H
6CH
3Si (OC
2H
5)
2) and AlCl
3Solution is raw material, the preparation covalent bond type inorganic organic composite flocculant.Covalent bond type inorganic organic composite flocculant is that inorganic component and organic constituent are compound with covalent linkage, total aluminium concentration 0.05～0.25mol/L, and Si/Al mol ratio 0.1～0.4, basicity 0.5～2.0, the pH value is 3.50～4.50.
Reaction structure formula of the present invention is:
Water in the reaction formula is from AlCl
3Water in water in the solution and the NaOH solution.Reaction back Al is a kind of polymeric form.
The preparation technology of covalent bond type inorganic organic composite flocculant is with γ-aminopropyl diethoxymethyl silane APDES and AlCl
3After solution mixed, adopting slowly, an alkaline process made covalent bond type inorganic organic composite flocculant.
Concrete preparation technology is as follows, in there-necked flask, presses Si/Al mol ratio 0.1～0.4, quantitatively adds AlCl
3Solution and γ-aminopropyl diethoxymethyl silane mixes the back and stirs fast under room temperature, adopts constant flow pump to drip NaOH solution, NaOH mole number and AlCl
3Ratio be 0.5～2.0, to basicity B=0.5～2.0, after the gained solution left standstill is treated complete reaction, promptly obtain covalent bond type inorganic organic composite flocculant.
The application of covalent bond type inorganic organic composite flocculant is used for turbidity removal, decolouring, de-oiling and the solid-liquid separation of water supply purification, wastewater treatment process.
The present invention compared with prior art has following advantage:
The organic constituent of 1 covalent bond type inorganic organic composite flocculant is the organo-functional group of γ-aminopropyl diethoxymethyl silane, links to each other with the Si atom by C-Si, and inorganic component is an aluminium salt, passes through Al-O-Si key (AlCl behind the aluminium salt hydrolysis
3Al links to each other with the O atom after the hydrolysis) link to each other with the Si atom, realized the compound of inorganic component and organic constituent with the covalent linkage form.
2 covalent bond type inorganic organic composite flocculants have the turbidity removal good decolorizing effect, characteristics such as best dispensing a wider range.
Embodiment
Enumerate 1 embodiment and 2 application examples below, the present invention is further specified, but be not limited thereto.
Example 1:
Covalent bond type inorganic organic composite flocculant, total aluminium concentration 0.2mol/L, the Si/Al mol ratio is 0.4, and basicity B is 2.0, and the pH value is 4.4.
The preparation method is as follows:
Quantitatively add 50mL respectively by predetermined Si/Al mol ratio in there-necked flask, concentration is the AlCl of 1.0mol/L
3The APDES of solution and 4.32mL.Stir fast under room temperature then, adopt constant flow pump slowly to drip 200mL, concentration is the extremely predetermined B value of NaOH solution of 0.5mol/L, i.e. NaOH mole number and AlCl
3Ratio be 2.0, titration time is 3 hours, gained solution left standstill question response fully after, promptly obtain the product that total aluminium concentration is 0.2mol/L.
1 of application example
The coagulation turbidity removal that the covalent bond type inorganic organic composite flocculant product of above example 1 preparation is used for the kaolin muddy water is handled, simultaneously and traditional aluminum salt flocculant---polymerize aluminum chloride (being called for short PAC, basicity 2.0) contrasts.Raw water turbidity is 90NTU, pH value 7.8.Result is listed in the table 1.
The different dosages of table 1 (in Al, mol/L), after covalent bond type inorganic organic composite flocculant example 1 is handled, the coagulation turbidity removal effect of the residual turbidity of water (NTU)
As can be seen from Table 1, the covalent bond type inorganic organic composite flocculant of the inventive method preparation has the turbidity removal effect more excellent than polymerize aluminum chloride.
2 of application example
The coagulation decoloration that the covalent bond type inorganic organic composite flocculant product of above example 1 preparation is used to contain the colored water of humic acid is handled, simultaneously and traditional aluminum salt flocculant---polymerize aluminum chloride (being called for short PAC, basicity 2.0) contrasts.Former colority of water represents that with the 370nm light absorption value its value is 0.250.The pH value is 6.0.Result is listed in the table 2.
The different dosages of table 2 (in Al, mol/L), after covalent bond type inorganic organic composite flocculant example 1 is handled, the coagulate decoloring effect of the residue colourity of water
As can be seen from Table 2, the covalent bond type inorganic organic composite flocculant of the inventive method preparation has the decolorizing effect more excellent than polymerize aluminum chloride, and the optimal coagulant dose scope is wideer.
Claims (4)
1. a covalent bond type inorganic organic composite flocculant is characterized in that raw material is organic γ-aminopropyl diethoxymethyl silane and inorganic aluminum chloride, and composite flocculation agent is AlCl
3And γ-aminopropyl diethoxymethyl silane is compound with covalent linkage, total aluminium concentration 0.05～0.25mol/L, and Si/Al mol ratio 0.1～0.4, basicity 0.5～2.0, the pH value is 3.50～4.50,
The reaction structure formula is:
2. by the preparation technology of the described covalent bond type inorganic organic composite flocculant of claim 1, it is characterized in that after γ-aminopropyl diethoxymethyl silane and liquor alumini chloridi mixing, adopting slowly, an alkaline process makes covalent bond type inorganic organic composite flocculant.
3. according to the preparation technology of the described covalent bond type inorganic organic composite flocculant of claim 2, it is characterized in that, press Si/Al mol ratio 0.1～0.4, under room temperature, stir fast after quantitatively getting liquor alumini chloridi and γ-aminopropyl diethoxymethyl silane mixture, adopt constant flow pump to drip NaOH solution, the NaOH mole number is 0.5～2.0 with the ratio of aluminum chloride, to basicity B=0.5～2.0, after the gained solution left standstill is treated complete reaction, promptly obtain covalent bond type inorganic organic composite flocculant.
4. by the application of the described covalent bond type inorganic organic composite flocculant of claim 1, be used for turbidity removal, decolouring, de-oiling and the solid-liquid separation of water supply purification, wastewater treatment process.
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| CN101298347B true CN101298347B (en) | 2010-06-02 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102897887A (en) * | 2012-11-09 | 2013-01-30 | 天津亿利科能源科技发展股份有限公司 | Polymer-containing oil-field wastewater treating agent |
| CN104085972B (en) * | 2014-07-22 | 2015-10-21 | 北京大学 | A kind of denitrogenation flocculation agent and its preparation method and application |
| CN108083543A (en) * | 2017-11-28 | 2018-05-29 | 北京大学深圳研究生院 | A kind of Dredged bed mud method for treating residual water of built-up flocculant and application built-up flocculant |
| CN108178262B (en) * | 2017-12-28 | 2021-01-01 | 陕西省石油化工研究设计院 | Inorganic-organic composite polymeric flocculant with high aluminum ion concentration |
| CN111573802B (en) * | 2020-05-08 | 2023-04-07 | 南京师范大学 | Hydrophobic modified organic/inorganic composite flocculant and preparation method and application thereof |
| CN113087220A (en) * | 2021-04-27 | 2021-07-09 | 同济大学 | Method for separating macromolecular organic pollutants in percolate concentrated solution by combined flocculation |
| CN115057508B (en) * | 2022-05-10 | 2023-06-23 | 同济大学 | Preparation method of quartz sand dead-weight flocculant |
| CN116813046B (en) * | 2023-06-30 | 2024-03-08 | 青岛水务集团有限公司 | Treatment method of landfill leachate concentrated solution |
| CN116621387B (en) * | 2023-06-30 | 2023-11-14 | 青岛水务集团有限公司 | Concentrated solution full-quantification treatment system and method |
| CN117699934B (en) * | 2024-02-06 | 2024-05-10 | 克拉玛依市弘智油田技术服务有限公司 | Water purifying agent and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3810843A (en) * | 1971-05-28 | 1974-05-14 | Gen Electric | Silicone-silica compositions |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3810843A (en) * | 1971-05-28 | 1974-05-14 | Gen Electric | Silicone-silica compositions |
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Application publication date: 20081105 Assignee: Beijing Ke Yi innovation environment Technology Co., Ltd. Assignor: Peking University Contract record no.: 2013990000272 Denomination of invention: Covalent bond type inorganic organic composite flocculant, preparation process and use thereof Granted publication date: 20100602 License type: Exclusive License Record date: 20130524 |
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